Carver R A, Borsetti A P, Kamps L R
J Assoc Off Anal Chem. 1978 Jul;61(4):877-83.
Finfish, shellfish, and crustacean samples are extracted with isopropanol and benzene; the extract is filtered and then concentrated. The extract, dissolved in hexane, is treated with oleum and extracted with aqueous alkali. The aqueous phase is acidified and extracted with petroleum ether-ethyl ether (1 + 1). The Kepone residue is determined by electron capture gas-liquid chromatography (GLC). Recoveries obtained by 8 laboratories from 15 species of finfish fortified at 0.02-0.23 ppm ranged from 37 to 107% with a mean +/- relative standard deviation of 79.4 +/- 14.5%. For oysters fortified at 0.01-0.10 ppm, recoveries range from 63 to 129% with a mean of 78.8 +/- 20.8%. For crustaceans fortified at 0.05-0.26 ppm, recoveries ranged from 52 to 110% with a mean of 78 +/- 16.4%. The approximate limits of quantitation for finfish and for shellfish and crustaceans are 0.02 and 0.05 ppm, respectively, under the GLC conditions used in this study.
将有鳍鱼、贝类和甲壳类动物样本用异丙醇和苯进行萃取；萃取液经过过滤后再进行浓缩。将溶解于己烷中的萃取液用发烟硫酸处理，然后用碱水溶液萃取。水相经酸化后用石油醚 - 乙醚（1 + 1）萃取。通过电子捕获气液色谱法（GLC）测定开蓬残留量。8个实验室对15种添加浓度为0.02 - 0.23 ppm的有鳍鱼进行回收率测定，回收率范围为37%至107%，平均回收率±相对标准偏差为79.4±14.5%。对于添加浓度为0.01 - 0.10 ppm的牡蛎，回收率范围为63%至129%，平均回收率为78.8±20.8%。对于添加浓度为0.05 - 0.26 ppm的甲壳类动物，回收率范围为52%至110%，平均回收率为78±16.4%。在本研究使用的GLC条件下，有鳍鱼以及贝类和甲壳类动物的近似定量限分别为0.02 ppm和0.05 ppm。
